Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'A. Clearfield' 'Jiang-Gao Mao' 'Zhike Wang' _publ_contact_author_name 'Prof A Clearfield' _publ_contact_author_address ; Prof A Clearfield Department of Chemistry Texas A & M University College Station TEXAS TX 77843 U S A ; _publ_contact_author_email 'CLEARFIELD@MAIL.CHEM.TAMU.EDU' _publ_section_title ; Building layered structures from hydrogen bonded molecular units and ID metal phosphonate chains: Synthesis, characterization and crystal structures of N,N'-dimethyl-N,N'-ethylenediamine-bis(methylenephosphonic acid), its Ni(II) and Pb(II) complexes ; data_maoc5 _database_code_CSD 195094 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 N2 O6 P2' _chemical_formula_weight 276.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n #(No. 14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.9401(15) _cell_length_b 10.456(2) _cell_length_c 8.4868(18) _cell_angle_alpha 90.00 _cell_angle_beta 112.844(4) _cell_angle_gamma 90.00 _cell_volume 567.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 292 _exptl_absorpt_coefficient_mu 0.400 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD ' _diffrn_measurement_method 'narrow frame method, hemisphere data' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 3330 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1279 _reflns_number_gt 1147 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.5430P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1279 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.09436(8) 0.30470(5) 0.40374(6) 0.0123(2) Uani 1 1 d . . . N1 N 0.3255(3) 0.46267(16) 0.2692(2) 0.0141(4) Uani 1 1 d . . . H11A H 0.3267 0.5449 0.2344 0.017 Uiso 1 1 calc R . . C1 C 0.5069(3) 0.44961(19) 0.4377(2) 0.0151(4) Uani 1 1 d . . . H1B H 0.6368 0.4598 0.4214 0.018 Uiso 1 1 calc R . . H1C H 0.5060 0.3650 0.4844 0.018 Uiso 1 1 calc R . . C2 C 0.1147(3) 0.44101(19) 0.2751(3) 0.0147(4) Uani 1 1 d . . . H2A H 0.0139 0.4292 0.1590 0.018 Uiso 1 1 calc R . . H2B H 0.0753 0.5178 0.3194 0.018 Uiso 1 1 calc R . . C3 C 0.3592(4) 0.3795(2) 0.1390(3) 0.0177(4) Uani 1 1 d . . . H3A H 0.4952 0.3960 0.1388 0.026 Uiso 1 1 calc R . . H3B H 0.2544 0.3979 0.0280 0.026 Uiso 1 1 calc R . . H3C H 0.3497 0.2913 0.1666 0.026 Uiso 1 1 calc R . . O1 O -0.1460(2) 0.28561(14) 0.34051(19) 0.0162(4) Uani 1 1 d . . . H1A H -0.1862 0.2391 0.2560 0.024 Uiso 1 1 calc R . . O2 O 0.1739(2) 0.35003(13) 0.58667(18) 0.0151(3) Uani 1 1 d . . . O3 O 0.2067(2) 0.19215(13) 0.36886(19) 0.0161(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0149(3) 0.0074(3) 0.0144(3) -0.00021(17) 0.0053(2) -0.00034(17) N1 0.0200(9) 0.0076(8) 0.0157(8) -0.0002(6) 0.0078(7) 0.0011(6) C1 0.0179(10) 0.0100(9) 0.0162(9) -0.0012(8) 0.0052(8) 0.0012(7) C2 0.0164(10) 0.0111(9) 0.0160(9) 0.0008(7) 0.0056(8) 0.0019(7) C3 0.0246(11) 0.0139(10) 0.0168(10) -0.0028(8) 0.0106(8) 0.0018(8) O1 0.0165(8) 0.0144(7) 0.0171(7) -0.0042(6) 0.0060(6) -0.0025(5) O2 0.0187(7) 0.0106(7) 0.0140(7) 0.0007(5) 0.0042(6) 0.0000(5) O3 0.0206(8) 0.0076(7) 0.0205(8) -0.0018(5) 0.0083(6) 0.0001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O3 1.5033(15) . ? P1 O2 1.5081(15) . ? P1 O1 1.5541(16) . ? P1 C2 1.834(2) . ? N1 C3 1.494(2) . ? N1 C1 1.500(3) . ? N1 C2 1.500(3) . ? C1 C1 1.521(4) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 P1 O2 115.98(9) . . ? O3 P1 O1 113.62(9) . . ? O2 P1 O1 108.11(8) . . ? O3 P1 C2 108.99(9) . . ? O2 P1 C2 106.66(9) . . ? O1 P1 C2 102.40(9) . . ? C3 N1 C1 109.73(16) . . ? C3 N1 C2 111.82(16) . . ? C1 N1 C2 115.01(16) . . ? N1 C1 C1 110.1(2) . 3_666 ? N1 C2 P1 116.02(13) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.498 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.091 data_mao15 _database_code_CSD 195095 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H20 N2 Ni O8 P2' _chemical_formula_weight 368.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n #(No. 13) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y, -z-1/2' _cell_length_a 8.302(7) _cell_length_b 9.042(7) _cell_length_c 9.932(8) _cell_angle_alpha 90.00 _cell_angle_beta 112.577(13) _cell_angle_gamma 90.00 _cell_volume 688.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 1.677 _exptl_absorpt_correction_type 'psi scan method' _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method 'Narrow frame method, hemisphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 4068 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.59 _reflns_number_total 1571 _reflns_number_gt 1328 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+1.0699P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1571 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1692 _refine_ls_wR_factor_gt 0.1655 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.2500 0.36650(9) -0.2500 0.0166(3) Uani 1 2 d S . . P1 P 0.15910(17) 0.28851(15) 0.01592(13) 0.0255(4) Uani 1 1 d . . . N1 N 0.0739(5) 0.1920(5) -0.2631(4) 0.0248(9) Uani 1 1 d . . . C1 C 0.1814(8) 0.0547(6) -0.2185(6) 0.0339(12) Uani 1 1 d . . . H1A H 0.1071 -0.0315 -0.2528 0.041 Uiso 1 1 calc R . . H1B H 0.2359 0.0497 -0.1130 0.041 Uiso 1 1 calc R . . C2 C -0.0040(7) 0.2193(7) -0.1536(6) 0.0325(12) Uani 1 1 d . . . H2A H -0.0531 0.1280 -0.1348 0.039 Uiso 1 1 calc R . . H2B H -0.0977 0.2908 -0.1919 0.039 Uiso 1 1 calc R . . C3 C -0.0644(7) 0.1736(8) -0.4097(5) 0.0395(14) Uani 1 1 d . . . H3A H -0.1392 0.0932 -0.4083 0.059 Uiso 1 1 calc R . . H3B H -0.0123 0.1527 -0.4788 0.059 Uiso 1 1 calc R . . H3C H -0.1316 0.2629 -0.4373 0.059 Uiso 1 1 calc R . . O1W O 0.0598(5) 0.5250(5) -0.2930(4) 0.0430(11) Uani 1 1 d . . . H1WA H 0.0438 0.5524 -0.2056 0.052 Uiso 1 1 d R . . H1WB H 0.0927 0.6106 -0.3337 0.052 Uiso 1 1 d R . . O11 O 0.2882(4) 0.3690(4) -0.0310(4) 0.0251(7) Uani 1 1 d . . . O12 O 0.2385(5) 0.1606(4) 0.1210(4) 0.0345(9) Uani 1 1 d . . . H12A H 0.2351 0.1797 0.2006 0.052 Uiso 0.50 1 calc PR . . O13 O 0.0607(6) 0.3920(5) 0.0805(4) 0.0381(10) Uani 1 1 d . . . H13A H 0.0210 0.4621 0.0253 0.057 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0158(4) 0.0269(5) 0.0077(4) 0.000 0.0050(3) 0.000 P1 0.0278(7) 0.0415(8) 0.0114(6) -0.0026(5) 0.0122(5) -0.0007(5) N1 0.027(2) 0.038(2) 0.0112(18) -0.0048(16) 0.0091(16) -0.0103(17) C1 0.056(3) 0.028(3) 0.021(2) -0.001(2) 0.019(2) -0.004(2) C2 0.025(2) 0.054(3) 0.021(3) -0.004(2) 0.013(2) -0.010(2) C3 0.036(3) 0.064(4) 0.012(2) -0.004(2) 0.001(2) -0.023(3) O1W 0.049(2) 0.059(3) 0.0203(19) 0.0020(18) 0.0127(17) 0.030(2) O11 0.0266(17) 0.0402(19) 0.0094(15) -0.0036(13) 0.0080(12) -0.0046(14) O12 0.050(2) 0.039(2) 0.0186(18) -0.0019(15) 0.0172(17) 0.0078(17) O13 0.049(2) 0.053(2) 0.021(2) 0.0039(16) 0.0240(18) 0.0188(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1W 2.052(4) 4_655 ? Ni1 O1W 2.052(4) . ? Ni1 O11 2.074(4) . ? Ni1 O11 2.074(4) 4_655 ? Ni1 N1 2.121(4) . ? Ni1 N1 2.121(4) 4_655 ? P1 O11 1.510(4) . ? P1 O12 1.528(4) . ? P1 O13 1.535(4) . ? P1 C2 1.819(5) . ? N1 C3 1.477(6) . ? N1 C2 1.484(6) . ? N1 C1 1.493(7) . ? C1 C1 1.495(11) 4_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Ni1 O1W 91.4(3) 4_655 . ? O1W Ni1 O11 88.76(14) 4_655 . ? O1W Ni1 O11 90.36(14) . . ? O1W Ni1 O11 90.36(14) 4_655 4_655 ? O1W Ni1 O11 88.76(14) . 4_655 ? O11 Ni1 O11 178.7(2) . 4_655 ? O1W Ni1 N1 171.69(15) 4_655 . ? O1W Ni1 N1 92.9(2) . . ? O11 Ni1 N1 84.08(14) . . ? O11 Ni1 N1 96.86(15) 4_655 . ? O1W Ni1 N1 92.9(2) 4_655 4_655 ? O1W Ni1 N1 171.69(15) . 4_655 ? O11 Ni1 N1 96.86(15) . 4_655 ? O11 Ni1 N1 84.08(14) 4_655 4_655 ? N1 Ni1 N1 83.8(3) . 4_655 ? O11 P1 O12 113.9(2) . . ? O11 P1 O13 113.0(2) . . ? O12 P1 O13 109.6(2) . . ? O11 P1 C2 104.1(2) . . ? O12 P1 C2 110.1(3) . . ? O13 P1 C2 105.7(3) . . ? C3 N1 C2 110.4(4) . . ? C3 N1 C1 110.4(4) . . ? C2 N1 C1 107.4(4) . . ? C3 N1 Ni1 113.6(3) . . ? C2 N1 Ni1 108.4(3) . . ? C1 N1 Ni1 106.3(3) . . ? N1 C1 C1 109.9(3) . 4_655 ? N1 C2 P1 110.9(3) . . ? P1 O11 Ni1 118.51(19) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.777 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.167 data_mao17 _database_code_CSD 195096 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H16 N2 O6 P2 Pb' _chemical_formula_weight 481.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 17.202(3) _cell_length_b 8.8751(14) _cell_length_c 8.2710(13) _cell_angle_alpha 90.00 _cell_angle_beta 105.014(3) _cell_angle_gamma 90.00 _cell_volume 1219.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brock _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 14.113 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method ; narrow frame method, hemisphere, 0.3deg/frame, 30s/frame ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 3670 _diffrn_reflns_av_R_equivalents 0.1056 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.24 _reflns_number_total 1384 _reflns_number_gt 1324 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+10.7684P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1384 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5000 0.52353(3) 0.7500 0.00856(12) Uani 1 2 d S . . P1 P 0.34279(8) 0.66688(15) 0.90694(17) 0.0104(3) Uani 1 1 d . . . N1 N 0.4126(3) 0.7572(5) 0.6542(5) 0.0094(8) Uani 1 1 d . . . C1 C 0.4553(3) 0.8872(6) 0.7490(7) 0.0118(10) Uani 1 1 d . . . H1A H 0.4502 0.8834 0.8630 0.014 Uiso 1 1 calc R . . H1B H 0.4305 0.9799 0.6984 0.014 Uiso 1 1 calc R . . C2 C 0.3340(3) 0.7328(6) 0.6935(7) 0.0117(10) Uani 1 1 d . . . H2A H 0.3033 0.6596 0.6155 0.014 Uiso 1 1 calc R . . H2B H 0.3041 0.8267 0.6767 0.014 Uiso 1 1 calc R . . C3 C 0.3978(3) 0.7837(6) 0.4715(7) 0.0134(10) Uani 1 1 d . . . H3A H 0.3649 0.8719 0.4407 0.020 Uiso 1 1 calc R . . H3B H 0.3706 0.6982 0.4115 0.020 Uiso 1 1 calc R . . H3C H 0.4482 0.7983 0.4441 0.020 Uiso 1 1 calc R . . O11 O 0.4191(2) 0.5721(5) 0.9526(5) 0.0149(8) Uani 1 1 d . . . O12 O 0.2663(2) 0.5812(4) 0.9060(5) 0.0139(8) Uani 1 1 d . . . O13 O 0.3545(2) 0.8047(5) 1.0258(5) 0.0156(8) Uani 1 1 d . . . H13A H 0.3108 0.8308 1.0388 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.00699(18) 0.01012(18) 0.00868(17) 0.000 0.00221(12) 0.000 P1 0.0055(6) 0.0133(6) 0.0126(6) -0.0005(5) 0.0028(5) 0.0002(5) N1 0.009(2) 0.0116(18) 0.0068(19) 0.0019(16) 0.0008(16) -0.0012(17) C1 0.007(2) 0.013(2) 0.016(2) -0.001(2) 0.0032(19) 0.0034(18) C2 0.006(2) 0.014(2) 0.012(2) 0.0016(19) -0.0028(18) -0.0003(19) C3 0.011(2) 0.018(2) 0.010(2) 0.005(2) 0.0009(19) 0.001(2) O11 0.0099(19) 0.0227(19) 0.0115(18) 0.0033(17) 0.0016(15) 0.0073(18) O12 0.0090(17) 0.0130(18) 0.021(2) -0.0028(15) 0.0067(16) -0.0039(15) O13 0.0074(17) 0.0204(19) 0.021(2) -0.0065(17) 0.0077(15) -0.0034(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O11 2.478(4) 6_657 ? Pb1 O11 2.478(4) . ? Pb1 N1 2.564(4) 6_657 ? Pb1 N1 2.564(4) . ? Pb1 O11 2.634(4) 2_564 ? Pb1 O11 2.634(4) 5_667 ? P1 O12 1.518(4) . ? P1 O11 1.522(4) . ? P1 O13 1.549(4) . ? P1 C2 1.829(5) . ? N1 C1 1.478(7) . ? N1 C3 1.485(6) . ? N1 C2 1.486(6) . ? C1 C1 1.535(10) 6_657 ? O11 Pb1 2.634(4) 5_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Pb1 O11 160.0(2) 6_657 . ? O11 Pb1 N1 71.40(14) 6_657 6_657 ? O11 Pb1 N1 92.16(14) . 6_657 ? O11 Pb1 N1 92.16(14) 6_657 . ? O11 Pb1 N1 71.40(14) . . ? N1 Pb1 N1 72.0(2) 6_657 . ? O11 Pb1 O11 71.23(14) 6_657 2_564 ? O11 Pb1 O11 115.71(16) . 2_564 ? N1 Pb1 O11 132.47(14) 6_657 2_564 ? N1 Pb1 O11 81.14(14) . 2_564 ? O11 Pb1 O11 115.71(16) 6_657 5_667 ? O11 Pb1 O11 71.23(14) . 5_667 ? N1 Pb1 O11 81.14(14) 6_657 5_667 ? N1 Pb1 O11 132.47(14) . 5_667 ? O11 Pb1 O11 142.4(2) 2_564 5_667 ? O12 P1 O11 114.5(2) . . ? O12 P1 O13 111.6(2) . . ? O11 P1 O13 108.5(2) . . ? O12 P1 C2 107.5(2) . . ? O11 P1 C2 105.5(2) . . ? O13 P1 C2 108.9(2) . . ? C1 N1 C3 110.3(4) . . ? C1 N1 C2 110.6(4) . . ? C3 N1 C2 108.6(4) . . ? C1 N1 Pb1 107.2(3) . . ? C3 N1 Pb1 112.0(3) . . ? C2 N1 Pb1 108.0(3) . . ? N1 C1 C1 111.4(4) . 6_657 ? N1 C2 P1 113.9(3) . . ? P1 O11 Pb1 121.9(2) . . ? P1 O11 Pb1 128.5(2) . 5_667 ? Pb1 O11 Pb1 108.77(14) . 5_667 ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 2.865 _refine_diff_density_min -4.911 _refine_diff_density_rms 0.411